Acetylated cellulose nanocrystal prepared through organic acid catalysis one-pot method

A cellulose and organic acid technology, applied in the field of functionalized polymer materials, can solve the problems of poor dispersion of cellulose nanocrystals, easy to agglomerate, etc., and achieve good degradability, good biocompatibility, good atomic economical effect

Inactive Publication Date: 2019-03-22
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the poor dispersion of cellulose nanocrystals, the tendency to agglomerate, and the need for further modification and modification, the present invention provides an alternative method, an organic acid-catalyzed one-pot method for the preparation of acetylated cellulose nanocrystals

Method used

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  • Acetylated cellulose nanocrystal prepared through organic acid catalysis one-pot method
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  • Acetylated cellulose nanocrystal prepared through organic acid catalysis one-pot method

Examples

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Embodiment 1

[0024] (1) Pretreatment of filter paper: crush the commercially available filter paper with a paper shredder, dry it in an oven at 105°C for 3 hours, and then grind it into a floc structure with a grinder for later use.

[0025] (2) Preparation of cellulose nanocrystals: (a) Weigh 5g of p-toluenesulfonic acid, 5.55g of water, and 50g of acetic acid, mix them, and soak 5g of filter paper powder prepared in step (1) in the solution overnight. (b) Set the rotation speed at 300r / min, react in a mechanically stirred water bath at 90°C for 90min, cool in an ice bath quickly, stir in an ice water bath for 2h, and then centrifuge to recover the acid solution. (c) The obtained solid was centrifuged and washed with deionized water, and the centrifugal speed was set at 9000r / min, centrifuged for 4min, and centrifuged several times until the conductivity of the supernatant was less than 50S / m. (d) Put the obtained suspension into a 8000-14000 dialysis bag, and dialyze with deionized water...

Embodiment 2

[0028] (1) Pretreatment of filter paper: crush the commercially available filter paper with a paper shredder, dry it in an oven at 105°C for 3 hours, and then grind it into a floc structure with a grinder for later use.

[0029] (2) Preparation of cellulose nanocrystals: (a) Weigh 5g of p-toluenesulfonic acid, 6.25g of water, and 25g of acetic acid, mix them, and soak 2.5g of filter paper powder prepared in step (1) in the solution overnight. (b) Set the rotational speed at 350r / min, react in a mechanically stirred water bath at 100°C for 60min, cool in an ice bath, and stir for 2.5h in an ice-water bath, then centrifuge to recover the acid solution. (c) The obtained solid was centrifuged and washed with deionized water, and the centrifugation speed was set at 8000r / min, centrifuged for 6min, and centrifuged several times until the conductivity of the supernatant was less than 50S / m. (d) Put the obtained suspension into a 8000-14000 dialysis bag, and dialyze with deionized wat...

Embodiment 3

[0031] (1) Pretreatment of filter paper: crush the commercially available filter paper with a paper shredder, dry it in an oven at 105°C for 3 hours, and then grind it into a floc structure with a grinder for later use.

[0032] (2) Preparation of cellulose nanocrystals: (a) Weigh 5g of p-toluenesulfonic acid, 8.33g of water, and 75g of acetic acid, mix them, and soak 7.5g of filter paper powder prepared in step (1) in the solution overnight. (b) Set the rotational speed at 400r / min, react in a mechanically stirred water bath at 80°C for 120min, cool in an ice bath, and stir for 3h in an ice-water bath, then centrifuge to recover the acid solution. (c) The obtained solid was centrifuged and washed with deionized water, and the centrifugation speed was set to 7000r / min, centrifuged for 8min, and centrifuged several times until the conductivity of the supernatant was less than 50S / m. (d) Put the obtained suspension into a 8000-14000 dialysis bag, and dialyze with deionized water...

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Abstract

The invention belongs to the field of functional high molecular materials and in particular relates to an acetylated cellulose nanocrystal prepared through an organic acid catalysis one-pot method. The acetylated cellulose nanocrystal is prepared by taking a mixed solution of organic acid and p-methylbenzenesulfonic acid as an acidolysis agent, and cellulose-containing substances including filterpaper powder, microcrystalline cellulose and the like as raw materials through the one-pot method. According to the method provided by the invention, decomposition and acetylation of the cellulose canbe carried out at the same time, so that the requirements of a plurality of reaction steps are eliminated; all the raw materials are industrial products and are cheap and easy to obtain, and the method is simple and reliable. The acetylated cellulose nanocrystal has high strength, a large specific surface area, good biocompatibility and degradability, so that the acetylated cellulose nanocrystalhas great potential application in the fields of reinforcing filler of polymers, optical materials, electrical materials, biomedical materials, medicine packages, food additives, cosmetics and the like.

Description

technical field [0001] The invention belongs to the field of functional polymer materials, and in particular relates to an organic acid catalyzed one-pot method for preparing acetylated cellulose nanocrystals. technical background [0002] As a ubiquitous polymer on the earth, cellulose has an annual output of 1.5×10 12 About tons [Khalil H PS A, Bhat A H, Yusra A F I. Green composites from sustainable cellulose enanofibrils: A review [J]. Carbohydrate Polymers, 2012, 87 (2): 963-979. Haafiz M K, Hassan A, Zakaria Z, et al.Isolation and characterization of microcrystallinecellulose from oil palm biomass residue[J].Carbohydrate Polymers,2013,93(2):628-634.], most of which are produced by photosynthesis and exist in the cell wall of plants. More and more researchers are studying how to efficiently utilize cellulose. Cellulose nanocrystals (CNC) are obtained by treating cellulose with different treatment methods, removing the non-crystalline region of cellulose and retaining ...

Claims

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Application Information

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IPC IPC(8): C08B15/02C08B3/06
CPCC08B3/06C08B15/02
Inventor 具本植刘治梅张淑芬
Owner DALIAN UNIV OF TECH
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